CN112299883A - High-temperature-resistant protective coating of silicon carbide heating element and preparation method thereof - Google Patents
High-temperature-resistant protective coating of silicon carbide heating element and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature-resistant protective coating of a silicon carbide heating element and a preparation method thereof, belonging to the technical field of preparation of high-temperature-resistant protective coatings2) And an in-situ sintering reaction of the coated slurry with titanium oxide (TiO)2) And zirconium oxide (ZrO)2) Or Yttria Stabilized Zirconia (YSZ) ceramic powder as a raw material. The high-temperature resistant protective coating of the silicon carbide heating element and the preparation method thereof provided by the invention take titanium oxide and zirconia or Yttria Stabilized Zirconia (YSZ) ceramic powder as raw materials, and a compact ceramic protective layer of silicon Zirconium Titanium Silicate (ZTS) is formed by ball milling pulping, coating and high-temperature sintering reaction, so that the oxidation resistance and corrosion resistance of the silicon carbide (SiC) heating element can be greatly improved, the process is simple, the cost is low, and the high-temperature resistant protective coating is suitable for large-scale industrial use.
Description
Technical Field
The invention relates to the technical field of preparation of high-temperature-resistant protective coatings, in particular to a high-temperature-resistant protective coating of a silicon carbide heating element and a preparation method thereof.
Background
Silicon carbide (SiC) ceramic materials have many excellent material properties, and are widely used in the fields of petroleum, chemical engineering, microelectronics, automobiles, aerospace, heavy machinery, atomic energy and the like, for example, silicon carbide ceramics are widely used in parts such as precision bearings and the like by utilizing the advantages of wear resistance, large elastic modulus, corrosion resistance and the like of the silicon carbide ceramic materials; the silicon carbide ceramic is widely applied to grinding in the field of machining by utilizing the advantages of wear resistance, high hardness and the like of the silicon carbide ceramic material; the silicon carbide ceramic material is widely applied to industrial high-temperature heating elements by utilizing the advantages of excellent electrical conductivity, high-temperature thermal stability and the like of the silicon carbide ceramic material, and various shapes can be prepared to meet the requirement of industry due to the good forming characteristic of the silicon carbide ceramic materialThe field multi-working condition use requirements; silicon carbide ceramic materials are also widely used in military equipment, protective layers for bulletproof armored vehicles, and the like. In a plurality of application fields of silicon carbide ceramic materials, the silicon carbide ceramic material is used as an industrial high-temperature heating element and is an important application. Under a certain working condition temperature, a layer of silicon dioxide (SiO) can be formed on the surface of the silicon carbide ceramic material through oxidation2) The silicon dioxide layer has certain oxidation resistance; when the working condition temperature is higher than 800 ℃, the silicon dioxide layer can form a porous structure to generate embrittlement and easily generate associated chemical reaction, so that the antioxidant protection effect is reduced or even lost; when the working condition temperature is higher than 1650 ℃, the silicon carbide (SiC) is converted from passive oxidation to active oxidation under the aerobic condition, which can cause the heating element to be seriously damaged, and particularly, under the severe working condition, the silicon carbide (SiC) ceramic material is easy to react with active gas, which causes oxidation and corrosion, and reduces or even loses the conductivity, thereby limiting the application of the silicon carbide (SiC) ceramic material under the high-temperature severe working condition. At present, no effective technical measures are available for processing the technical current situation that the conductivity of a silicon carbide (SiC) ceramic material is reduced or even lost due to passive oxidation and corrosion under severe working conditions. Therefore, a high temperature resistant protective coating of a silicon carbide heating element with simple process, low cost and stable performance and a preparation method thereof are needed.
Summary of the invention
The invention aims to solve the problem that a silicon carbide (SiC) ceramic material is easy to react with active gas under severe working conditions to cause oxidation and corrosion and reduce or even lose conductivity under the existing severe working conditions, and provides a high-temperature resistant protective coating of a silicon carbide heating element, which has the advantages of simple process, low cost and stable performance, and a preparation method thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a high-temperature resistant protective coating for silicon carbide (SiC) heating elements, the coating being formed by pre-oxidizing silicon dioxide (SiO) on the surface of the silicon carbide (SiC) heating element2) And the coated slurry is subjected to in-situ sintering reactionThe slurry is made of titanium oxide (TiO)2) And zirconium oxide (ZrO)2) Or Yttria Stabilized Zirconia (YSZ) ceramic powder as a raw material.
A preparation method of a high-temperature resistant protective coating of a silicon carbide (SiC) heating element comprises the following steps:
step 1: silicon carbide (SiC) heating element pretreatment
Cleaning the surface of a silicon carbide (SiC) heating element, putting the silicon carbide (SiC) heating element into an oven to be dried for 2 hours at the temperature of 150 ℃, and then putting the silicon carbide (SiC) heating element into a high-temperature furnace to be heated for 2 to 5 hours at the temperature of 1000 ℃ in the air or oxygen atmosphere to form a white silicon oxide layer on the surface;
step 2: preparation of coating slurries
Weighing 50-60 g of titanium oxide (TiO)2) And 40 to 50g of zirconium oxide (ZrO)2) Or adding yttria-stabilized zirconia (YSZ) ceramic powder into a zirconia ceramic ball-milling tank with the volume of 500-1000 mL, adding 200-400 mL of grinding balls, 250-500 mL of purified water and 10-20 g of PVB adhesive into the zirconia ceramic ball-milling tank, sealing and filling the mixture into a planetary ball mill, operating at 500RPM for 24 hours, and filtering to remove zirconium balls to form 250-500 mL of slurry with the solid content of 40%;
and step 3: preparation of the coating
Uniformly coating the slurry formed in the step 2 on the silicon oxide layer formed in the step 1 by adopting a brush coating mode, wherein the coating thickness is 100-150 mu m, and naturally airing for 4 hours or heating and drying for 2 hours at 150 ℃;
and 4, step 4: in-situ sintering of coatings
And (3) placing the silicon carbide (SiC) heating element coated with the coating formed in the step (3) into a high-temperature sintering furnace, heating to 1200-1400 ℃ at the heating rate of 10-15 ℃/min, and preserving heat for 1-2 hours to generate a Zirconium Titanium Silicate (ZTS) protective layer on the surface.
In the above method for preparing the high temperature resistant protective coating of the silicon carbide (SiC) heating element, in the step 2, zirconium oxide (ZrO) is used2) The purity is more than or equal to 99.5 percent.
In the step 2, the yttria-stabilized zirconia ceramic powder is added to the high temperature resistant protective coating of the silicon carbide (SiC) heating elementY of (A) is2O3The content is 3-5%.
In the step 2, the ratio of the grinding balls to the grinding balls is D10: D6: D4: 2:5: 3.
In the above preparation method of the high temperature resistant protective coating for the silicon carbide (SiC) heating element, in the step 2, the PVB content of the PVB binder is 3-6W%.
Compared with the prior art, the invention has the following beneficial effects:
1. the high-temperature resistant protective coating of the silicon carbide heating element provided by the invention takes titanium oxide and zirconium oxide or Yttria Stabilized Zirconia (YSZ) ceramic powder as raw materials, and a compact ceramic protective layer of silicon Zirconium Titanium Silicate (ZTS) is formed by ball milling pulping, coating and high-temperature sintering reaction, so that the oxidation resistance and corrosion resistance of the silicon carbide (SiC) heating element can be greatly improved, the process is simple, the cost is low, and the high-temperature resistant protective coating is suitable for large-scale industrial use;
2. the invention provides a high-temperature resistant protective coating of a silicon carbide heating element and a preparation method thereof, wherein the surface of the silicon carbide (SiC) heating element is pre-oxidized to form porous silicon dioxide (SiO)2) Filling gaps with ultrafine particles of titanium oxide and zirconium oxide or Yttria Stabilized Zirconia (YSZ) ceramic powder, and sintering at high temperature in situ to form a compact ceramic protective layer of Zirconium Titanium Silicate (ZTS), so that gas is completely prevented from diffusing to a silicon carbide (SiC) surface layer, the silicon carbide protective layer is not easy to fall off, the performance is stable, embrittlement and associated chemical reactions are effectively reduced, and the antioxidant protection effect is improved;
3. compared with the existing preparation methods (such as plasma spraying, sputtering, chemical vapor deposition and the like), the high-temperature-resistant protective coating of the silicon carbide heating element and the preparation method thereof have the advantages of simple process flow, no need of special equipment, low cost and wide market application value.
Drawings
FIG. 1 is a flow chart of the process principle of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the following detailed description is combined with the embodiments of the invention: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a process are given, but the scope of the present invention is not limited to the following embodiments.
The invention is further described below with reference to the accompanying drawings:
referring to FIG. 1, a refractory protective coating for a silicon carbide (SiC) heating element is provided, the coating comprising silicon dioxide (SiO) pre-oxidized on the surface of the silicon carbide (SiC) heating element2) And an in-situ sintering reaction of the coated slurry with titanium oxide (TiO)2) And zirconium oxide (ZrO)2) Or Yttria Stabilized Zirconia (YSZ) ceramic powder as a raw material.
A preparation method of a high-temperature resistant protective coating of a silicon carbide (SiC) heating element comprises the following steps:
step 1: silicon carbide (SiC) heating element pretreatment
Cleaning the surface of a silicon carbide (SiC) heating element, putting the silicon carbide (SiC) heating element into an oven to be dried for 2 hours at the temperature of 150 ℃, and then putting the silicon carbide (SiC) heating element into a high-temperature furnace to be heated for 2 to 5 hours at the temperature of 1000 ℃ in the air or oxygen atmosphere to form a white silicon oxide layer on the surface;
step 2: preparation of coating slurries
Weighing 50-60 g of titanium oxide (TiO)2) 40 to 50g of zirconium oxide (ZrO)2) Or adding yttria-stabilized zirconia (YSZ) ceramic powder, 200-400 mL of grinding balls, 250-500 mL of purified water and 10-20 g of PVB adhesive into a zirconia ceramic ball milling tank with the volume of 500-1000 mL, sealing and filling the zirconia ceramic ball milling tank into a planetary ball mill, operating at 500RPM for 24 hours, filtering and removing the zirconium balls to form 250-500 mL of slurry with the solid content of 40%, wherein Y in the yttria-stabilized zirconia (YSZ) ceramic powder2O3The content of the PVB adhesive is 3-5%, the ratio of the grinding balls is D10: D6: D4: 2:5:3, and the content of PVB in the PVB adhesive is 3-6W%;
and step 3: preparation of the coating
Uniformly coating the slurry formed in the step 2 on the silicon oxide layer formed in the step 1 by adopting a brush coating or a coating mode, wherein the coating thickness is 100-150 mu m, and naturally airing for 4 hours or heating and drying for 2 hours at 150 ℃;
and 4, step 4: in-situ sintering of coatings
And (3) placing the silicon carbide (SiC) heating element coated with the coating formed in the step (3) into a high-temperature sintering furnace, heating to 1200-1400 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 hours, naturally cooling along with the furnace, generating a Zirconium Titanium Silicate (ZTS) protective layer on the surface, adding Yttria Stabilized Zirconia (YSZ) ceramic powder into coating slurry to improve the mechanical property and the thermal expansion property of the protective layer, and adding a PVB adhesive into the coating slurry to facilitate the adjustment of the thickness of the coating and the formation of the coating.
The process principle flow, as shown in the attached figure 1, comprises the following reaction steps:
first, a silicon dioxide (SiO) formed by pre-oxidizing the surface of a silicon carbide (SiC) heating element2) The reaction principle is shown in formula (1),
second, silicon dioxide (SiO) formed by pre-oxidizing the surface of the silicon carbide (SiC) heating element2) Titanium oxide (TiO) in layer and coated slurry2) And zirconium oxide (ZrO)2) Reacting, and performing high-temperature in-situ sintering to form a compact Zirconium Titanium Silicate (ZTS) protective layer, wherein the reaction principle is shown in formula (2).
Example 1
Step 1, cleaning the surface of a silicon carbide (SiC) heating rod to remove impurities on the surface, and placing the silicon carbide (SiC) heating rod in a high-temperature furnace at 1000 ℃ in an air atmosphere for heating pretreatment for 3 hours to form a white silicon oxide layer on the surface of the silicon carbide (SiC) heating rod.
Step 2, weighing 50g of titanium oxide and 50g of zirconium oxide, wherein the purity of the zirconium oxide is more than or equal to 99.5%, adding the zirconium oxide into a zirconium oxide ceramic ball milling tank with the volume of 500mL, adding grinding balls with the volume of 200mL and the proportion of D10: D6: D4: 2:5:3, adding 250mL of purified water, adding 10g of PVB adhesive, wherein the content of PVB is 3-6W%, sealing and filling the mixture into a planetary ball mill, operating for 24 hours at 500RPM, and filtering to remove the zirconium balls to form 250mL of coating slurry with the solid content of 40%.
And 3, uniformly coating the slurry prepared in the step 2 on the silicon oxide layer formed by pretreating the silicon carbide (SiC) heating rod in the step 1 by adopting a brush coating method or a coating method, wherein the coating thickness is 100 mu m, and naturally airing for 4 hours.
And 4, placing the silicon carbide (SiC) substrate coated in the step 3 into a high-temperature sintering furnace, heating to 1350 ℃ at a heating rate of 10 ℃/min in an air atmosphere for surface sintering, sintering for 1 hour, and naturally cooling along with the furnace.
And (4) taking out the silicon carbide (SiC) heating rod formed in the step (4), and electrifying 220V alternating current to electrically heat the silicon carbide (SiC) heating rod to 1200 ℃ for 72 hours, wherein the surface of the silicon carbide (SiC) heating rod is not oxidized.
Example 2
Step 1, cleaning the surface of a silicon carbide (SiC) heating rod to remove impurities on the surface, and placing the silicon carbide (SiC) heating rod in a high-temperature furnace at 1000 ℃ in an air atmosphere for heating pretreatment for 4 hours to form a white silicon oxide layer on the surface of the silicon carbide (SiC) heating rod.
Step 2, weighing 60g of titanium oxide and 40g of zirconium oxide, wherein the purity of the zirconium oxide is more than or equal to 99.5%, adding the zirconium oxide into a zirconium oxide ceramic ball milling tank with the volume of 500mL, adding grinding balls with the volume of 200mL and the proportion of D10: D6: D4: 2:5:3, adding 250mL of purified water, adding 10g of PVB adhesive, wherein the content of PVB is 3-6W%, sealing and filling the mixture into a planetary ball mill, operating at 500RPM for 24 hours, filtering and removing the zirconium balls to form 250mL of coating slurry with the solid content of 40%.
And 3, uniformly coating the slurry prepared in the step 2 on the silicon oxide layer formed by pretreating the silicon carbide (SiC) heating rod in the step 1 by adopting a brush coating method or a coating method, wherein the coating thickness is 150 mu m, and naturally airing for 4 hours.
And 4, placing the silicon carbide (SiC) substrate coated in the step 3 into a high-temperature sintering furnace, heating to 1350 ℃ at a heating rate of 10 ℃/min in an air atmosphere for surface sintering, sintering for 0.5 hour, and naturally cooling along with the furnace.
And (4) taking out the silicon carbide (SiC) heating rod formed in the step (4), and electrifying 220V alternating current to electrically heat the silicon carbide (SiC) heating rod to 1200 ℃ for 72 hours, wherein the surface of the silicon carbide (SiC) heating rod is not oxidized.
In summary, the basic principles, main features and advantages of the present invention have been shown and described, which are merely examples of the present invention, and are not intended to limit the scope of the present invention. The present invention is not limited to the above-described embodiments, and all equivalent changes and modifications in the shape, structure, characteristics and spirit of the present invention described in the claims should fall within the scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A high temperature resistant protective coating for a silicon carbide (SiC) heating element, the coating comprising silicon dioxide (SiO) pre-oxidized on the surface of the silicon carbide (SiC) heating element2) And an in-situ sintering reaction of the coated slurry with titanium oxide (TiO)2) And zirconium oxide (ZrO)2) Or Yttria Stabilized Zirconia (YSZ) ceramic powder as a raw material.
2. A preparation method of a high-temperature resistant protective coating of a silicon carbide (SiC) heating element is characterized by comprising the following steps:
step 1: silicon carbide (SiC) heating element pretreatment
Cleaning the surface of a silicon carbide (SiC) heating element, putting the silicon carbide (SiC) heating element into an oven to be dried for 2 hours at the temperature of 150 ℃, and then putting the silicon carbide (SiC) heating element into a high-temperature furnace to be heated for 2 to 5 hours at the temperature of 1000 ℃ in the air or oxygen atmosphere to form a white silicon oxide layer on the surface;
step 2: preparation of coating slurries
Weighing 50-60 g of titanium oxide (TiO)2) And 40 to 50g of zirconium oxide (ZrO)2) Or Yttria Stabilized Zirconia (YSZ) ceramicsAdding ceramic powder into a zirconia ceramic ball milling tank with the volume of 500-1000 mL, adding 200-400 mL of grinding balls, 250-500 mL of purified water and 10-20 g of PVB adhesive into the zirconia ceramic ball milling tank, sealing and filling the mixture into a planetary ball mill, operating at 500RPM for 24 hours, and filtering to remove zirconium balls to form 250-500 mL of slurry with the solid content of 40%;
and step 3: preparation of the coating
Uniformly coating the slurry formed in the step 2 on the silicon oxide layer formed in the step 1 by adopting a brush coating mode, wherein the coating thickness is 100-150 mu m, and naturally airing for 4 hours or heating and drying for 2 hours at 150 ℃;
and 4, step 4: in-situ sintering of coatings
And (3) placing the silicon carbide (SiC) heating element coated with the coating formed in the step (3) into a high-temperature sintering furnace, heating to 1200-1400 ℃ at the heating rate of 10-15 ℃/min, and preserving heat for 1-2 hours to generate a Zirconium Titanium Silicate (ZTS) protective layer on the surface.
3. A method of preparing a high temperature resistant protective coating for a silicon carbide (SiC) heating element according to claim 2, wherein: in said step 2, zirconium oxide (ZrO)2) The purity is more than or equal to 99.5 percent.
4. A method of preparing a high temperature resistant protective coating for a silicon carbide (SiC) heating element according to claim 2, wherein: in the step 2, Y in the yttria-stabilized zirconia ceramic powder2O3The content is 3-5%.
5. A method of preparing a high temperature resistant protective coating for a silicon carbide (SiC) heating element according to claim 2, wherein: in the step 2, the ratio of the grinding balls is D10: D6: D4: 2:5: 3.
6. A method of preparing a high temperature resistant protective coating for a silicon carbide (SiC) heating element according to claim 2, wherein: in the step 2, the PVB content of the PVB adhesive is 3-6W%.
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